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Rapid synthesis method of Sn-doped MFI zeolite molecular sieve

A technology for zeolite molecular sieves and synthesis methods, applied in molecular sieves and base exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of large amount of structure-directing agent, hindering crystallization of molecular sieves, long crystallization time, etc. problems, to achieve the effect of easy industrial application, high crystallinity, and short crystallization time

Pending Publication Date: 2021-10-08
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to Sn 4+ The ionic radius of tin is relatively large, and tin salts are very easy to hydrolyze in aqueous solution. Directly introducing tin salts into the synthesis system of molecular sieves will greatly hinder the crystallization of molecular sieves, resulting in a large amount of structure-directing agents in the synthesis process of heteroatom molecular sieves containing tin. , long crystallization time and poor repeatability

Method used

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  • Rapid synthesis method of Sn-doped MFI zeolite molecular sieve
  • Rapid synthesis method of Sn-doped MFI zeolite molecular sieve
  • Rapid synthesis method of Sn-doped MFI zeolite molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0020] According to the molar ratio: Sn / SiO 2 =0.02, structure directing agent / SiO 2 =0.18, Alkali / SiO 2 =0.02,H 2 O / SiO 2 =6.6, the mass ratio is: silicate-1 molecular sieve / SiO 2 =0.04, polymer / SiO 2 =0.11, at first 13.6g fumed silica, 0.2g NaOH, 33.6g tetrapropyl ammonium hydroxide (mass fraction is 25% aqueous solution), 2mL deionized water, 1.8gSnCl 4 ·5H 2 O mixed, ground for 30 minutes, added 0.6g silicate-1 molecular sieve, continued to grind for 30 minutes, then added 1.5g of polydiallyldimethylammonium chloride (PDDA), continued to grind for 30 minutes, and the resulting gel was transferred to a polytetrafluoroethylene In a stainless steel high-pressure hydrothermal reaction kettle lined with ethylene, crystallize in a constant temperature drying oven at 200°C for 3h, cool to room temperature, centrifuge and wash with water until neutral, dry in a constant temperature drying oven at 80°C for 24h, and then transfer to a horse Sn-doped MFI zeolite molecular siev...

Embodiment 2

[0022] According to the molar ratio: Sn / SiO 2 =0.05, structure directing agent / SiO 2 =0.24, Alkali / SiO 2 =0.02,H 2 O / SiO 2 =6.4, the mass ratio is: silicate-1 molecular sieve / SiO 2 =0.12, polymer / SiO 2 =0.32, firstly mix 10.0g sodium silicate, 0.05g NaOH, 10.0g tetrapropylammonium hydroxide (25% aqueous solution), 2mL deionized water, 1.5g SnCl 4 ·5H 2 O mixed, grinded for 30 minutes, added 0.6g silicate-1 molecular sieve, continued to grind for 30 minutes, then added 1.6g polyethylene terephthalate (PET), continued to grind for 30 minutes, and the resulting gel was transferred into a polytetrafluoroethylene In a lined stainless steel high-pressure hydrothermal reaction kettle, crystallize in a constant temperature drying oven at 190°C for 10h, cool to room temperature, centrifuge and wash to neutrality, dry in a constant temperature drying oven at 80°C for 24h, and then transfer to a muffle furnace Calcined at 550°C for 6h to obtain Sn-doped MFI zeolite molecular sieve...

Embodiment 3

[0024] According to the molar ratio: Sn / SiO 2 =0.04, structure directing agent / SiO 2 =0.2, Alkali / SiO 2 =0.11,H 2 O / SiO 2 =8, the mass ratio is: silicate-1 molecular sieve / SiO 2 =0.05, polymer / SiO 2 =0.17, first 30.0g tetraethyl orthosilicate, 0.50g NaOH, 19.0g tetrapropylammonium hydroxide (25% aqueous solution), 2mL deionized water, 1.6g SnCl 4 ·5H 2 O mixing, grinding for 30min, adding 0.5g silicate-1 molecular sieve, continuing grinding for 30min, then adding 1.6g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123), continuing grinding for 30min , the resulting gel was transferred to a stainless steel high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene liner, crystallized in a constant temperature drying oven at 170 ° C for 10 h, cooled to room temperature, centrifuged and washed to neutrality, and placed in a constant temperature drying oven Dry at 80°C for 24h, and then transfer to muffle furnace for calcinatio...

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Abstract

The invention discloses a rapid synthesis method of a Sn-doped MFI zeolite molecular sieve. The method comprises the following steps: uniformly mixing and stirring a silicon source, a structure-directing agent (such as tetrapropylammonium hydroxide, tetrapropylammonium bromide, tetraethylammonium hydroxide and the like), alkali (such as sodium hydroxide, potassium hydroxide and the like), a crystal seed silicate-1 molecular sieve, water and a tin source to form gel. adding a certain amount of polymer into the gel, and heating for a very short time under certain conditions to prepare the Sn-containing MFI structure molecular sieve with the framework. The synthesized Sn-doped MFI zeolite molecular sieve has very high crystallinity and Lewis acidity and also shows very high catalytic reaction performance in related catalytic reactions. The method is very simple in preparation process, good in repeatability and easy for industrial application.

Description

technical field [0001] The invention belongs to the technical field of synthesis of zeolite molecular sieves, in particular to a rapid synthesis method of Sn-doped MFI (Sn-MFI) zeolite molecular sieves. Background technique [0002] Heteroatom molecular sieves containing Sn in the framework have very strong Lewis acidity, and have attracted widespread attention due to their excellent catalytic performance in numerous acid-catalyzed reactions such as Bayer-Villiger oxidation, glucose isomerization, and hydration of epoxy compounds. . However, due to Sn 4+ The ionic radius of tin is relatively large, and tin salts are very easy to hydrolyze in aqueous solution. Directly introducing tin salts into the synthesis system of molecular sieves will greatly hinder the crystallization of molecular sieves, resulting in a large amount of structure-directing agents in the synthesis process of heteroatom molecular sieves containing tin. , long crystallization time and poor repeatability....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/04
CPCC01B39/48C01B39/04C01P2002/72C01P2004/03C01P2004/61
Inventor 刘忠文袁恩辉李梦宋永红江金强李果刘昭铁
Owner SHAANXI NORMAL UNIV
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